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A kind of preparation method of high molecular weight polyacrylamide

A technology of polyacrylamide and high molecular weight, which is applied in the production of bulk chemicals and can solve the problems of high energy consumption, cross-linking and denaturation of products, etc.

Active Publication Date: 2018-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of high energy consumption in the product purification process in the prior art and the cross-linking and denaturation of the product caused by the post-treatment process, and achieve the purpose of saving energy, reducing emissions and reducing energy consumption, the present invention provides a supercritical CO 2 Method for preparing high molecular weight and high purity polyacrylamide in medium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 12.10 g of acrylamide, 0.0005 g of azobisisobutylamidine hydrochloride, and 0.002 g of ammonium persulfate into a 100 ml autoclave; seal it and blow nitrogen for 10 minutes to exclude oxygen, then add 0.002 g of sodium bisulfite solution.

[0030] Fill with CO using a high pressure pump 2 Make it reach the critical state, carry out the polymerization reaction, the temperature is 0 ℃, the pressure is 14MPa, the reaction time is 8 hours; then reduce the temperature and reduce the pressure to obtain a white wet block, and the measured intrinsic viscosity is 19.54dl / g. Monomer content determination Acrylamide monomer residual 1.7%.

[0031] The intrinsic viscosity [η] in the present invention is the value measured according to GB12005.1-89 Acrylamide Copolymer Intrinsic Viscosity Determination Method, and this value is used to characterize the molecular weight of the polymer.

Embodiment 2

[0033] Add 12.10 g of acrylamide to a 100 ml autoclave, add 0.002 g of azobisisobutylamidine hydrochloride, and 0.002 g of ammonium persulfate; seal it and blow nitrogen for 10 minutes to exclude oxygen, then add 0.002 g of sodium bisulfite.

[0034] Fill with CO using a high pressure pump 2 Make it reach the critical state, carry out the polymerization reaction, the temperature is 0 ℃, the pressure is 14MPa, the reaction time is 8 hours; then reduce the temperature and reduce the pressure to obtain a white wet block, and the measured intrinsic viscosity is 14.26dl / g. Monomer content determination Acrylamide monomer residual 0.7%.

Embodiment 3

[0036] Add 12.10 g of acrylamide, 0.0005 g of azobisisobutylamidine hydrochloride, and 0.002 g of ammonium persulfate into a 100 ml autoclave; seal it and blow nitrogen for 10 minutes to exclude oxygen, then add 0.002 g of sodium bisulfite.

[0037] Fill with CO using a high pressure pump 2 Make it reach the critical state, carry out the polymerization reaction, the temperature is 0°C, the pressure is 14MPa, the reaction time is 8 hours; then the reactor is raised to 80°C and kept for 1 hour.

[0038] Then open the outlet valve and inject CO with a high-pressure pump 2 , keep the pressure at 11MPa, resolver temperature at 55°C, autoclave at 50°C, and slowly resolve the CO passing through the wet flowmeter 2 The flow rate is 40 liters (normal pressure state) / hour. Finally, while cooling, slowly depressurizing, the measured intrinsic viscosity of the product is 23.80dl / g. The monomer content was determined to be 0.03% of the residual acrylamide monomer.

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Abstract

The invention provides a preparation method of high-molecular-weight polyacrylamide. The method includes the steps of performing segmented polymerization to acrylamide and an initiator in a high-pressure kettle with a supercritical CO2 medium to obtain high-molecular-weight polyacrylamide; and then performing supercritical CO2 fluid extraction to extract small-molecular monomers which are incompletely reacted to obtain high-purity polyacrylamide. The product is pure and is free of follow-up treatment. The reaction medium is toxic-free and environment-friendly. The preparation method is economic and practical, and is green and environment-friendly.

Description

technical field [0001] The present invention relates to a kind of preparation method of polyacrylamine, more specifically, relate to a kind of using oxidation-reduction initiation system in supercritical CO 2 A method for preparing high-molecular-weight polyacrylamide in medium, and using supercritical fluid extraction technology to improve the purity of polyacrylamide. Background technique [0002] Acrylamide (PAM) is an important class of water-soluble polymers. It has special physical and chemical properties. It is easy to obtain various modified products with branched chain or network structure through grafting or crosslinking. It is widely used in petroleum, Metal and chemical mining, water treatment, textile, paper and other industries. The current methods of synthesizing polyacrylamide mainly include aqueous solution polymerization, inverse emulsion polymerization, inverse microemulsion polymerization, suspension polymerization, precipitation polymerization and so on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/56C08F220/58C08F220/56C08F2/00C08F4/40C08F4/34C08F4/04C08F6/00
CPCY02P20/54
Inventor 孙汝柳张建新马英陈静君单薇杨天予刘瞻
Owner CHINA PETROLEUM & CHEM CORP
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